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Allyl bromide → Isoprene butadiene

HRID 859839
ノート
印刷プレビュー

反応式

HRID 859839 の反応式
[CH2:1]=[CH:2][CH:3]=[CH2:4].[H-].[CH2:6]([Al+]CC(C)C)C(C)C.[Nd].C(Br)C=C>[Nd].CCCCCC>[CH2:1]=[CH:2][C:3](=[CH2:6])[CH3:4].[CH2:1]=[CH:2][CH:3]=[CH2:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7841Allyl bromideHCID 78451,3-ButadieneHCID 23934Neodymium2 回HCID 21225700Diisobutylaluminumhydride2 回

生成物 1

HCID 168288Isoprene butadiene収率 87%

試薬・触媒・溶媒 2

HCID 23934Neodymium触媒
HCID 8058
Hexane
溶媒
3 回

反応条件

温度
20 °C

実験手順

In this experiment, an isoprene-butadiene copolymer rubber was prepared using an alcohol modified neodymium catalyst system. In this procedure, a one gallon (3.78 liter) reactor was charged with 1,214 grams of hexane containing 81.3 grams of butadiene and 558.43 grams of 1.23 molar diisobutylaluminum hydride (DIBAH) in hexane, (i.e., 25% weight percent DIBAH). The reactor was maintained at 20° C. by cooling. N-butanol (11.16 grams) was added with stirring. After stirring for thirty minutes, 107.5 grams of 10.1% neodymium solution (neodymium neodecanoate) diluted with 160 grams of dry hexane, was charged to the reactor. The solution was stirred for another thirty minutes after which time 18.2 grams of allyl bromide was added. The cooling was stopped and the solution was allowed to warm up. A delayed exothermic reaction was noted. After twenty minutes, bring the solution temperatures to about 10° C. above ambient temperature. When the temperature ultimately dropped, the catalyst solution was aged by heating at 65° C. for ninety minutes. The catalyst prepared had a [butanol-DIBAH]Nd-allyl bromide-butadiene molar ratio of [2-13]-1-2-20, respectively, and a concentration of 0.025 molarity with respect to the neodymium.

後処理

  1. temperatureby cooling
  2. stirringAfter stirring for thirty minutes
  3. additionwas charged to the reactor
  4. additionwas added
  5. temperatureto warm up
  6. customA delayed exothermic reaction
  7. waitAfter twenty minutes
  8. customto about 10° C.
  9. customabove ambient temperature
  10. additionWhen the temperature ultimately dropped
  11. temperatureby heating at 65° C. for ninety minutes
  12. customThe catalyst prepared

出典と根拠

ORDレコード
ord-f70ae264a46a4a7a988d9097e1cf441c
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07153805B2

反応ノート

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